Process of combining titanium with iron.



iJnTTTnn STaTns PATENT FFICE.

AUGUSTE J. ROSSI, OF NEW YORK, N. Y., ASSIGNOR OF ONE-HALF TO JAMESMACNAUGHTON, OF TAHAWUS, NEV YORK.

PROCESS OF COMBINING TITANIUM WITH IRON.

SPECIFICATION forming part of Letters Patent No. 713,802, dated November18, 1902.

Application filed March 3, 1902. Serial No. 96,453. (No specimens.)

To all? whom it may concern:

Be it known that I, Aueosrn J. ROSSI, a citizen of the United States,residing in the borough of Manhattamcity, county, and State of New York,have invented certain new and useful Improvements in Processes ofCombining Titanium with Iron, of which the following is a specification.

The object of my invention is to produce processes by the assistance ofwhich predetermined and moderate amounts of pure metallic titanium maybe introduced into iron for industrial purposes with uniformity, ease,and the certainty of securing a homogeneous product, and to enable theseends to be obtained, so far as the iron-founder is concerned withoutdisturbing the usual conditions or procedures with which the averageworkman is now familiar-4. 8., without any special or novel preparationor manipulation by him of ingredients or treatment thereof with any morethan the present ordinary skill of his calling involved in, say, thefamiliar mixing of different grades of pig-iron in the cupola or inoperations involving the production of steel in the converter or openhearth.

I have discovered that the alloys of titanium and iron, for which UnitedStates Letters Patent No. 609,466 were granted to me August 23, 1898,and which alloys are characterized as containing not less than five percent. of titanium, are practically infusible per 86 under the ordinarytemperatures sufficient to melt iron or steel, and that in those casesin which my said last-mentioned alloys are employed for seasoning ironwith titanium the latter becomes incorporated in the resulting productby dissolving at the temperatures mentioned in the bath of molten ironor in contact with it analogously to the way in which platinum, likewiseinfusible per 36 at such temperatures, is known to dissolve in a bath ofmolten iron or to fuse in contact with it, whereby. may be produced aniron containing platinum. Therefore in order to insure success in theseasoning or titanizing of iron by the use of my said alloys containingabove five per cent. of titanium, and likewise the desired homogeneityof the product, these alloys must preliminarily be reduced to thepowdered state, or at least broken into small fragments, thus involvingundesirable expense, owing to their hard and refractoryeharacter,or,again,in certain cases as, for instance, when operating inthe ladle stirring of the mixture becomes likewise req uisite, all ofwhich necessitates special preparation and treatment by the workmen,involving some inconvenience, the exercise of perhaps more than hisusual skill and attention, and thus more or less undesirable eX- pense,and this is especially the case when the operations involved areconducted upon moderate amounts of metal in the smaller foundries andplants. One of the causes contributing to render these manipulationsnecessary under the circumstances mentioned consists, doubtless, in thecomparatively low specific gravity of the alloy of iron and titaniumwhen high in percentage of titauium,the specific gravity of titaniumbeing for instance 4.90, of an alloy containing ten per cent. oftitanium 5.60, of cast-iron 7, and of iron 7.78.

My present processes comprise as an essential preliminary the productionof an alloy of iron and titanium containing the latter in what my recentexperiments and discoveries have demonstrated to be the requiredproportions for the purposes mentionedthat is to say, in excess of twoand not to exceed five per centum of titanium. This new alloy Idesignate my special titanic pig. This I produce by supporting a mixtureof ingredients containing such proportions of titanic acid, of iron, orof iron oxids and of carbon as to result in a pig-iron having therequisite proportion of titanium and subjecting the mixture until therequisite reactions have been thereby accomplished to the intense heatproduced by the electric currentsay a heat of 3,500 Fahrenheit.

It will be understood that the titanie ..a,cid in the mixture abovereferred to may be in troduced in any convenient form-as, for instance,as contained in titanifergus iron ore tile.

of electrical device capable of producing the results described may beemployed-as, for instance, a Siemens furnace of the type described asearly 187 9or I have, for instance, used successfully for this purpose agraphite furnace or crucible properly insulated by an outside lining ofrefractory materials, such as magnesia bricks or the like, properlysecured by means of tie-rods, buckstaffs, and the like, the cruciblebeing properly connected with one of the poles of the current by meansof bus-bars, cables, or the like. Into this crucible was charged themixture referred to,a more specific illustration of which will be givenpresently. Over this charge I lowered a large carbon or bunch of carbonsconstituting the anode properly connected with the positive pole of thecurrent, the said anode being so disposed as to admit of its beinggradually raised or lowered by any convenient mechanism foraccomplishing that purpose. The current being turned on was passedthrough the materials to be reduced. The anode being of smaller diameterthanthe aperture of the crucible additions could be made to the chargefrom time to time as the reduction proceeded and the level of themixture sank in the crucible. After the charge, with its additions, hasbeen sufficiently exposed to the action of the current and the resultinghigh temperatures my special titanic pig is cast into proper moldsthrough a suitable opening provided at the bottom of the crucible andthe slag run out thereafter analogously to the similar practice involvedin the production of pig-iron in onpolas and blast-furnaces, after whichthe cruble or furnace is charged again as before and the operationrepeated indefinitely.

I have successfully produced my special titanic pig by using as one ofthe ingredients of the charge titaniferous iron ore containing on anaverage titanic acid, fifteen; oxid of iron, eighty; silica, 2.50;alumina, 1.50; magnesia, one; lime, trace; phosphorous, 0.017; sulfur,0.045. As this ore, however, contained nine per cent. titanium, beingtoo large a percentage for the purpose of producing the special titanicpig, I added in this instance a proper proportion of anothernon-titaniferous iron ore containing silica, 5.90; oxid of iron,eighty-five; alumina, 3.50; lime,

3.60; magnesia, 1.90; sulfur, 0.052; phosphorous, 0.07. As thetitaniferous ore in this instance contained fifty-six per cent. iron andnine per cent. titanium and the nontitaniferous ore contained fifty-sixper cent. iron and no titanium, I mixed one hundred pounds of the formerand two hundred and thirty pounds of the latter with the expectation ofsecuring by the process above de scribed and after allowing for lossesunavoidable in all metallurgical operations a resulting pig containingsome four per cent. of titaniumsay theoretically 4.30 per cent.-including carbon and silicon in the pig metal. The said ores properlypulverized were mixed with the requisite quantity of carbon, preferablyin the form of charcoal powder, necessary to secure the reduction of theoxids of iron and titanium, or, say, about sixty-five pounds ofcharcoal, and were charged into the crucible or electric furnace, asabove described, with about ten pounds of caustic lime added to themixture, in lieu of which I might have added its equivalent inlimestone.

The resulting pig metal produced by the treatment of the aforesaidmixture by the process above described contained silicon, 1.90;titanium,4.09; carbon,5.26; iron by diff., 88.75; total, one hundred.

It will be observed that instead of using in admixture with thetitaniferous ore an ore free from titanium, as above described, for thepurpose of reducing the percentage of titanium in the mixture to theproper figure for the purposes of my special titanic pig there mightwith equally beneficial results be substituted for the non-titaniferousores and in the required proportions ordinary pig-iron free fromtitanium.

As further illustrating the entire practicability of regulating withcertainty and exactness the percentage of titanium in the resulting pigby proportioning the respective ingredients of the charge uponatheoretic basis, I will add that in similar operations I have foundthat a mixture which would theoretically yield a titanic pig containing3.80 per cent. titanium treated as above described resulted in apig-iron containing 3.68 per cent. titanium; also, that on similarlytreating another mixture which would theoretically yield astitanic pigcontaining4.38 percent. titanium I obtained 4.28 per cent. titanium inthe pig, and from another mixture which should have yielded 2.80 percent. titanium I obtained 2.65 per cent. in the resulting pig-iron.

My special titanic pig having been produced as aforesaid, the next stepin my present process consists in utilizing it for the seasoning ortitanizing of iron containing no titanium. It is manifest that should myspecial titanic pig contain, say, less than two per cent. of titanium itwould prove scarcely available for the purposes in hand on anyindustrially economical basis, since, among other reasons, too great abulk thereof would be required to produce the requisite seasoning, and Iam therefore of the opinion that it must prove necessarily preferable inall instances that the percentage of titanium should be not less thanfour per cent. The seasoning required is accomplished by introducinginto the metal to be seasoned, while either cold in the charge or inmolten condition, the requisite proportion of my special titaniferouspig, which, among other things, owing to its percentage of titanium, asbefore explained, will under the ordinary and usual temperaturesrequired for the melting of iron employed in foundry-work and withoutpreliminary treatment or other manipulation melt with the same facilityas the ordinary non-titaniferous pig-iron with which it is associated.-

To secure the required titanizing of iron, for instance, my specialtitanic pig is charged solid into the cupola and in its original andunbroken form as pigs or ingots, (the same IIO as any other pig-iron nottitanic,) together with the pig-iron to be seasoned with titanium, carebeing taken to regulate the quantity of the titanic pig according to itspercentage of titanium and the total mass of the mixture, so as tosecure in the product the required percentage of titanium. The cupola isthen run in all respects in the ordinary manner, including theemployment of the same temperatures as in the case of ordinary iron,tapped, as usual, the resulting product flow ing out into the ordinaryreceiving-ladle, from which the pouring-ladles are filled for anypurpose of casting whatsoever, or if steel is to be made the contents ofthe cupola t'. 6., the molten titanized pig-ironare run directly intothe converter. Again, if my special titanic pig is desired to be used inthe openhearth furnace it is in the required quantity charged into thatalso, together with the noutitanic pig-iron, and the mixture treated inall respects according to the usual practices of such furnaces the sameas though no titanic pig were being smelted.

I am aware that pig-iron produced from titaniferous ores under suchtemperatures as are attainable in the blast-furnace has been claimed tocontain sometimes some titanium; but the proportion of the latter thusattainable has been invariably very small, hardly reaching a fewhundredths of one percentum, more exceptionally a few tenths, andWhenever, and abnormally and fortuitously only, such quantities as oneoreven one and onehalf per cent. oftitianium in iron'have been observed inthe products of experimental work or even of the blast-furnacethepresence thereof has been due not to the direct reducing action ofthe carbon on the titanic oxid, since carbon cannot at the temperaturesof the blastfurnace secure such reduction, which requires the intenseheat of a powerful current, but to indirect causes, irregular,unreliable, dependent upon special or accidental conditions, such as areuncontrollable by the founder and which may often interfere with theproper and regular running of the furnace. So far as I am informed allefforts to introduce pure metallic titanium into iron in greaterproportion than two per centum by the treatment of the ores in crucibleswithout the use of the electric current have failed. In fact, in manycases no trace of titanium has been discoverable by analysis in theso-called titanic product, and even when such a percentage has beensupposed to have been observed the analysis has shown that the titaniumwas not present as pure metallic titanium, as in the case of my specialtitanic pig, butin combination with carbon and nitrogen, as nitride orcyano nitride of titanium, being products which have long previouslybeen mistaken for titanium and the presence of which tends further todemonstrate that the reduction of the oxid of titanium at temperaturesattainable in the crucible by a fire or even in the blast-furnace is notdue to a direct action of carbon on the titanic oxid, but to somespecial accidental, uncontrollable, uncertain, and unreliableconditions, it being notable that the percentage of titanium in the orethus treated has noinfluence whatever upon the amount of titanium thusfortuitously found in the resulting pig. I do not wish, therefore, to beunderstood as claiming as any part of my present invention either theproduction or use of iron containing titanium derived by processes otherthan that hereinafter specifically claimed.

What I claim as new, and desire to secure by Letters Patent, is thefollowing, viz:

1. Theprocess ofcombining homogeneously with iron a certainpredetermined percentage of titanium which consists first in bringingtogether a mixture of titanic acid and iron, with carbon sufficient todeoxidize the titanic oxids, the proportion of titanic acid to theentire mixture being regulated so as to secure in the product derivedfrom the next step not less than two per centum nor as much as fivepercentum of titanium,next supporting the said ingredients, and while sosupported subjecting them to an. intense heat say not less than 3,500Fahrenheit, until the iron and the titanium resulting from thedeoxidization of the titanic acid, are thoroughly molten andhomogeneously commingled, next withdrawing the said molten mixture, fromthe said temperature, and allowingit to solidify; next, reducing tomolten state, while suitably supported and by application of thetemperatures usually required to melt the iron, both the iron to betitanized and the quantity of said solidified mixture required to impartto the resulting final product the required percentage of titanium, andcontinuing the said support subject to said last-mentioned temperatureuntil the constituent titanium has been melted and homogeneouslydistributed throughout the mass and finally withdrawing the said productfrom the said temperature and allowing it to solidify substantially asand for the purposes described.

2. The process ofcombining homogeneously with iron a certainpredetermined percentage of titanium which consists first in bringingtogether titaniferous iron ore,with carbon sufficient to deoxidize theiron and titanic 0xids, the proportion of titanic acid to the entiremixture being regulated so as to secure in the product derived from thenext step not less than two per centum nor as much as five per centum oftitanium, next supporting the said ingredients, and while so supportedsubjecting them to an intense heat say not less than 3,500 Fahrenheit,until the iron, resulting from the'deoxidization of the oxid of iron,and the titanium, from the deoxidization of the titanic acid, arethoroughly molten and homogeneously commingled, next withdrawing thesaid molten mixture from the said temperature and allowing it tosolidify, next reducing to molten state, while suitably supported and byapplication of the tempera tures usually required, both the iron to betitanized and the quantity of said solidified mixture required to impartto the resulting final product the required percentage of titanium, andcontinuing the said support subject to said last-mentioned temperatureuntil the constituent titanium has been melted and homogeneouslydistributed throughout the mass and finally Withdrawing the said productfrom the said temperature and allowing it to solidify substantially asand for the purposes described.

3. The process of titanizing iron Which consists first in producing apig-iron characterized as containing a percentage of titaniumsufiiciently low to insure the melting of' the titanium at the meltingtemperature of the iron and sufficiently high to effect the requiredtitanizing by the use of an industrially economic minimum of said pig,that is to say a pig containing not less than two per cent. nor morethan five per cent. of titanium;

next, combining the iron to be titanized with the said titaniferous pigin the proportions necessary to produce the required percentage oftitanium in the resulting product and melting the iron and thetitaniferous pig together, substantially as and for the purposesdescribed.

4. The process of producing a pig-iron containing a predeterminedproportion of titanium fusible under the ordinary melting temperaturesof pig-iron, that is to say not to exceed five per cent. of titaniumwhich consists in supporting titaniferous iron ore having the requisiteproportion of titanic acid in the presence of carbon and subjecting themixture to an intense heat say not less than 3,500 Fahrenheit until abath of molten iron is produced by the dioxidization of the iron oxidand until the titanium has been reduced and melted and a homogeneousmolten mixture of iron and pure metallic titanium secured substantiallyas and for the purposes described.

AUGUSTE J. ROSSI.

Witnesses:

WALTER D. EDMONDS, PHILIP C. PEoK.

